Title A compact cubic anvil high pressure apparatus

Author(s) Osugi, Jiro; Shimizu, Kiyoshi; Inoue, Kazuo; Yasunami, Kazuo

Citation The Review of Physical Chemistry of Japan (1964), 34(1): 1-6

Issue Date 1964-11-05

URL http://hdl.handle.net/2433/46842

Right

Type Departmental Bulletin Paper

Textversion publisher

Kyoto University

The Review of Physical Chemistry of Japan Vol. 34 No. 1 (1964)

THE REl'rEw Or PnyalCAl. CrtE3llarRl' OF JAPAF, Vor.. 34, ICo. 1, 1964

A COMPACT CUBIC ANVIL HIGH PRESSURE APPARATUS

Bv--]IRO V]UGI. Ktvosrtr Sxrastzv, Knzvo Ieove asn KazvoYasvxastt

The compact cubic anvil apparatus for generating to 100kb in a pyrophyllite

cube was devised and the calibration curve of pressure was determined.

The external ram force applied to only one axis is converted to six equal

components of force and the six anvils are forced to advance equally to the

center of pyrophyllite cube by the functions of the tetragonal bipyramidal

guide blocks and the trapezoid end bloc], of the Lour anvils located horizon-

tally and [hen throughout the pyrophyllite cube except its outer paz[ is com-

pressed homogeneously with increasing pressure. The calibration curve of pressure was determined by [he aid of phase

transitions of Bi I-II, TI II-III, Ba II-III and Bi V-VI. The hydrostatic pres-

sure [o IOOkb can be generated in a pyrophyllite cube with good efbciency, [hat

is, the load loss by gaskets of pyrophyllite is comparatively small.

Introduction

As the devices for generating static high pressures over 20 kb, the following three types are most im-

portant; piston-cylinder, opposed flat anvils and multiple anvil apparatus. In these devices, the multiple anvil apparatus is more suitable for hydrostatic compression. In this apparatus, it is necessary to form

the space of the regular polyhedron by [be flat faces of multiple anvils and to keep this geometrical

condition for increasing pressure by equally advancing anvils toward the geometrical center of the

polyhedron. The letrabedral anvil high pressure apparatus was first reported by H. T. Hallt) in 1918. This

apparatus consists of tour independent hydraulic rams to apply force to the faces of a tetrahedron of

pyrophyllite. Recently. the special anvil guide devicez) was installed on the head of ram in order to equalize the advance of each anvil.

Another type of the multiple anvil apparatus was developed by the researchers of the U. S. National

Bureau of Standardsa>. This equipment employs an assembly in which external force is applied only to

one of the four anvils and wedge reaction forces act on the remaining three anvils through the tetrahed-

ron of pressure transmitting medium.

The present apparatus employs an assembly in wbich the external ram force is applied only to one

vertical axis and is converted to act too along the other two recutangular axes of cubic pyrophyllite by

means of the inner surfaces of the upper aad lower pyramidal guide blacks installed on the Lead of press

(Received October 26,1964) 1) H. T. Hall, Reu. Sci. Instr., 29, 267 (1938)

?) H. T. Hall, ibid., 33, 1278 (1962) 3) E. C. Lloyd, U. 0. Hutton and D. P. johnsan, 1. Res, Nof. Bur. Stand., 63 C, 39 (1939)

The Review of Physical Chemistry of Japan Vol. 34 No. 1

2 J. Osugi, K. Shimizq K. moue and K Y"asunami

ram and the four trapezoid end blocks of anvils. Thus, the advance of all the anvils is automatically

synchronized so that the cubic pyrophyllite is compressed hydrostatically. \ioreover, this compact ap-

paratus has the advantages of the rapid adjustment and the easy manipulation.

(1964)

Photo. 1

pump up to

Construtlionand Operation

shows the whole assembly of this cubic apparatus which consists of the lower pressure oil

125 kg/cmz, the intensifier up to 2100 kg/cm~ and the cubic anvil apparntus in place in the

s~ ~ t ' + ~ -.~:

,}

e~o~

:-a! _yt

w

b Photo. 1

r

N

Pigh p

F~

.~~+ ~;

t .,

T' ~ ~

i

~" pressure assembly of compact cubic anvil

I

f~

Photo.

~`-

2 Nest of cubit anvil apparatus

iF

The Review of Physical Chemistry of Japan Vol. 34 No. 1 (1964)

A Compact Cubic Anvil High Pressure apparatus 3

1200 tons press rams. Photo.2 shows the cubic nest. of tungsten carbide anvis. The edge-length of the

flat face of the anvil is 10 mm, or 15 mm. Figs. 1 and 2 illustrate the general principle and the details of

the construction of this apparatus. The upperand lower guide blocks of SNCiv18 steel in JIS areattached

to the heads of the press ram,, the diameter of which is 2 SO mm. The inner surface of these guide blocks

is just as the tetragonal bipyramid with B=4i` as shown in Fig. 1. The two of the si.. anvils are along

the center line of this bipyramid and are fined opposite to each other on the bottom of each guide black.

The other four anvils are horizontally located on the mid points of the square edgesof hpyramid. This

results in the formation of a cubit nest by the flat Faces of sis anvils. As shown in Fig. 2. the vertical

e

/ '

;r~

1

.+

\ \

f ~

I J

euiJe blrcJ:

O

B

?aloe a~:~~i~.

:~~ ,

i

-; a~~~i c

guide blak

///Fig. 1 Principle of compact cubic snvil apparatus Fig. 2

• . ~ ~ ~ . . ~

Vertical crass section of compact cubic anvil

apparatus

n~e~~ n

cross section of the end block of these four anvils is in the shape of trap_zoid. These two oblique planes

(B=45-) of the end block of the four anvils are in contact with the inner surface of the bipyramidal guide blocks with tefion sheets inserted. In this way, the external ram force, which is applied to only one vertical

axis, is converted to the six equivalent components of force which act on the cubic pyrophyllite along

the three recutangular aces and the flat faces of thesis anvils ace then forced [o advance equally toward

the center of cube and always to form the cube with increasing pressure. This is illustrated in Fig. 3. The

movement of the anvils compressing a copper cube (12Smm edge-length) was measured by the dial

gauges. 'The advances of all the anvils are-automatically equalized with increasing pressure. The distribution of pressure in the pyrophyllite cuhe was tested by two methods. The pyrophyllite

cube was divided into twoequal parts and the fine wire mesh of copper was inserted. The assembly,

after being coated with iron oxide, was compressed ton load of 90 tons corresponded to 62.i kb (calibration

pressure). Photo. 3 shows the patterns of mesh before loading and after unloarding, which illustrate the homogeneity of compression throughout the cube except in its outer part. The other was the_simultane-

ous recording of the phase transition of three bismuth chips which were inserted in the pyrophyllite

The Review of Physical Chemistry of Japan Vol. 34 No. 1 (1964)

4 J, Osugi, K Shimizq K. moue and K. I'asunami

0.tl

4A e e

c

n. 'a

ns

r

I' .r~

Photo. 3o o m ao nn

Gauec prcsvm (YS'~7

Fig, 3 Movements of anvils with increasing pressure

Origin of ordinate is at the final

position o[ an anvil face.

cube along the three recutangular axes. These results are shown in Figs. 4 and i. The differences of tran-

sition pressure and in the time axis of the chart among the three chips are little in both cases of

loading and unloading.l'herzfore, i[ iscertain that the pyrophylli[e cube is compressed homo3eneously

in this apparatus.

q ~.. ..

u

~N

~.~f 11f

~I

_ a ~

!• ~ ~

Patterns of a fine wire mesh of copper before loading (:1) and after unloading B)

an

C

~~ e

v

lY

~~

i~~ ~-n-m

T

5 3.

j 111 '; Y

'

I

HI f-II-111

z

o~ o ~m ms m o m ~ s u x~

Gauae pxeswre (kg/ao') Time (mivl

Fig.4 Phase transition of three bismuth chips placed Fig.S Phasetransition of three bismuth chips placed in pyrophyllite cube along three recutangular io pyrophyllite cube along three recutangular

axes; X, Y and Z-Resistaace vs Pressure saes; X, Y and Z-Resistance vs Time

The guide blocks are insulated from the press rams with teflon. The anvils are mutually insulated

with teflon and polycarbonate and each anvil is provided electric terminal for physical measurements.

The Review of Physical Chemistry of Japan Vol. 34 No. 1 (1964)

A Compact Cubic Anvil High Pressure Apparatus 5

Pressure Calibration

The press load required to produce a given pressure in the pyrophyllite cube has been determined

by the aid of phase transitions of Bi I-II (25.4 kb), TI II-III (3i kb). Ba II-III (59kb)and Bi V-VI

(S9kbr> which are detected by the sharp changes in electrical resistance. \'ow, in this experiment, the anvil with edge-length of IOmm was used. e1s the solid pressure transmitting medium, pyrophyllite

(hydrous aluminum silicate) obtained from the American Lava Company a~as used. The initial edge-length of pyrophyllite cube was about 25 per cent larger than the edge-length of the am~il face. The sample

foil with about 0.08 mm in thickness, 0.5 mm in width and g mm in length was placed, in parallel with

.a

~ss S

$ sa a'

to

Ni Idl-I[I

Fig. 6

Im In ~ ru xo Gauae pressure /kpJrnFl

Phase transition of IIi I-II and II-IIl

ss

_!

?]

X23

21

5 s

uo

n n-m

~~

~.n

na n-m

8

,~

Fiq.

rso-- sao sx Gauge Preaare (kg/em'/

Phase transition of Ba

quo

II-III

High

~a

rso

F 16•

Gauge

Phase

~a >~ presare /kg,'cnr/

transition of T1 II-IlI

.~

u

a

au

E 20

s H 3` r

re is

4) F. P, Bundy, Bu[terwarths, London

"lfadern 1'ery Pressure

IA L-O

Fig. 9

Tecsniquer

ri; I-rt-m & tt. v-vt

9l W QO Gauac Vressure kg/un~

Pbase transition of Bi I-II, II~III

" edited by R . H. Weatorf, ]r., p.

and V-VI

I9 (1962),

The Review of Physical Chemistry of Japan Vol. 34 No. 1 (1964)

6 ]. Osugi, );. Shimiau, £ Iaoue and S. Pasunami

the surface, on the semi cube of pyrophyllite. The sur(ate of the pyrophyllite cube was coated with

iron oxide powder after construction. As to the changes in electrical resistance of the sample, the

potential drop, appling constant small current 2cross the sample, was measured as a function of

pressure by the potentiometer.

Pig. fi shows the resistance change of bismuth (99.959x) with pressure. The sharp drops in resist-

ance is due to the Bi I-II transition occurring at 2i.4 kb. The rise in resistance following the sharp drop

is due to Bi II-lII Cransition occurring at 2i kb. Some hysteresis are observed on unloading.

The phase transition of thallium (99.99A;) at 37 kb is shown in Pig. 7. Hysteresis is present as in

the case of bisnmtb.

The making of barium foil sample is difficult because of the oxidation of barium metal. The pre-

paration of the sample is as follow;. The new surface of barium metal (99.9°6) exposed by filing was

um

1

p GO v d

3U

m

lia I1r11[

~ '1'I II -III

L'i 1-II

Bi V-V]

_r

FIg. 10 Calihration curx•e of pressure

-~-: This experiment -+-: Graf's value obtained by py-

rophyllite dried at 90'C -t-: Graf's value obtained by as•

received pyrophyllite

O "LI/ JO M/ 80 IOU t?O IJU Calculated pressure (kb)

covered with vacuum grease and pressed in thin foil.'Fhe greased sample of a thin foil was [hen cut iota

proper dimension. The transition is shown in Fig. S. The third transition of bismuth in electrical resistance is shown in Pig. 9.

The calibration curve based on these results is shown in Fig. 10. The real pressure in the pyro-

phyllitecube are plotted versus the calculated load preuure. The points can be connected by a straight

line which does not pass through the origin. These results ace in good agreement with the data obtained

by R. B. Graf and B. C. Deatonsl using tetrahedral pyrophyllite dried at 90-C and show that the load

loss by gaskets of pyrophyllite is comparatively small.

The authors Gave great pleasure in expressing their sincere thanks to the Department of Education

for the Grant in Aid. The authors would like to thanL• &obe Steel IVorks. Ltd. and Sumitomo Electric

Industries, Ltd. for their aid. The Labosatory of Playsicnl CkemisL>y

Kyoto University

Kyoto. lapmr

3) R. B: Graf and B. C. Dea[oq Nature, 197, 678 (1963)